KR100349983B1 - Method for the Preparation of Sulfur-Soap - Google Patents
Method for the Preparation of Sulfur-Soap Download PDFInfo
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- KR100349983B1 KR100349983B1 KR1019990020130A KR19990020130A KR100349983B1 KR 100349983 B1 KR100349983 B1 KR 100349983B1 KR 1019990020130 A KR1019990020130 A KR 1019990020130A KR 19990020130 A KR19990020130 A KR 19990020130A KR 100349983 B1 KR100349983 B1 KR 100349983B1
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Abstract
본 발명은 지방산을 황화나트륨(Na2S)으로써 중화함으로써 소지(素地)비누를 제조함과 동시에 황화나트륨중의 유황을 원소유황으로 유리시켜 소지비누에 초미립의 유황분말을 자연발생적으로 균일하게 분산하도록 한 유황비누의 제조방법에 관한 것이다.The present invention neutralizes fatty acids with sodium sulfide (Na 2 S) to produce soy soap and release sulfur in sodium sulfide as elemental sulfur to uniformly produce ultra-fine sulfur powder naturally in soy soap. The present invention relates to a method for producing sulfur soap to be dispersed.
따라서 본 발명은 초미립의 유황분말로 인하여 유황비누의 약효를 증대시킬 수 있도록 한 것이다.Therefore, the present invention is to increase the efficacy of sulfur soap due to the ultra-fine sulfur powder.
Description
본 발명은 유황비누의 제조방법에 관한 것으로 더욱 상세하게는 본 발명은 지방산을 황화나트륨(Na2S)으로써 중화함으로써 소지(素地)비누를 제조함과 동시에 황화나트륨중의 유황을 원소유황으로 유리시켜 소지비누에 초미립의 유황분말을 자연발생적으로 균일하게 분산하도록 한 유황비누의 제조방법에 관한 것이다.The present invention relates to a method for producing sulfur soap, and more particularly, the present invention is to prepare a base soap by neutralizing fatty acid with sodium sulfide (Na 2 S) and at the same time liberated sulfur in sodium sulfide as elemental sulfur. The present invention relates to a method for producing sulfur soap, in which the ultra-fine sulfur powder is naturally and uniformly dispersed in the base soap.
비누의 제조방법은 사용원료에 따라 2가지로 대별할 수 있다. 즉, 유지를 원료로 하여 알칼리 수용액으로 가수분해하여 비누를 제조하는 방법인 증비법(蒸沸法)과 지방산을 원료로 하여 알칼리 수용액으로 중화하여 비누를 제조하는 방법인 중화법(中和法)이 있다.Soap manufacturing methods can be divided into two types depending on the raw materials used. That is, the thickening method, which is a method of producing soap by hydrolyzing with aqueous alkali solution using fat as a raw material, and the neutralization method, which is a method of producing soap by neutralizing with aqueous alkali solution using fatty acid as a raw material. There is this.
본 발명에서는 중화법을 이용하여 유황비누를 제조하는 방법을 제공하고자 한다.In the present invention, to provide a method for producing sulfur soap using the neutralization method.
유황비누는 여드름 등과 같은 피부병 치료를 위한 약용비누로 널리 쓰이고 있는데 종래의 제조방법에서는 우지 비누화시 또는 지방산 중화시 유황분말을 원료에 단순히 배합함으로써 유황분말을 소지비누에 분산시켜 왔다.Sulfur soap is widely used as a medicated soap for the treatment of skin diseases such as acne. In the conventional manufacturing method, sulfur powder is dispersed in the soap by simply blending sulfur powder in raw material during saponification of Uji saponification or fatty acid neutralization.
유황은 입자가 미세할수록 약효가 강하므로 입자가 미세할수록 유황의 배합량을 줄일 수 있고 또한 입자가 미세할수록 피부와 접촉하는 면적이 증대되어 동일한 양으로는 미세입자가 굵은 입자에 비하여 약효가 크다.Sulfur is more effective as the finer particles, so the finer particles can reduce the amount of sulfur compounded, and the finer the particles, the greater the area of contact with the skin.
그러나 미세 입도를 가진 유황분말을 얻기 위하여서는 기계적 분쇄에 의존할 수 밖에 없으나 유황분말을 기계적으로 초미립으로 분쇄하는 데에는 엄청난 동력이 소요되거나 또는 현실적으로 아예 불가능한 실정에 있다.However, in order to obtain sulfur powder having a fine particle size, it has no choice but to rely on mechanical pulverization. However, mechanically grinding sulfur powder into ultra-fine particles requires tremendous power or is not practically possible at all.
또한 종래의 제조방법에서는 유황분말을 소지비누에 단순히 기계적으로 혼합하여 분산시켜 왔으나 균일한 분산이 불충분한 문제점이 있어 왔다.In addition, in the conventional manufacturing method, the sulfur powder has been mechanically mixed and dispersed in the soap, but there has been a problem of insufficient uniform dispersion.
본 발명에서는 유황을 화학적 방법으로 소지비누에 유리시킴으로써 초미립의 유황분말을 얻을 수 있고 초미립의 유황분말을 소지비누에 자연발생적으로 균일하게 분산할 수 있도록 하며 또한 초미립의 유황분말로 인하여 약효를 증대시킨 유황비누를 제공하고자 한다.In the present invention, the sulfur is released in the soap by chemical method to obtain ultra fine sulfur powder, and the ultrafine sulfur powder can be naturally and uniformly dispersed in the soap by the ultra fine sulfur powder. To provide increased sulfur soap.
본 발명에서는 황화나트륨(Na2S)을 지방산의 중화제로 사용하여 소지비누를 제조함과 동시에 황화나트륨 중의 유황을 초미분의 유황분말로 유리시키고 유리된 유황분말을 기계적 조작없이 자연발생적으로 균일하게 분산하도록 한 것이다.In the present invention, sodium sulfide (Na 2 S) is used as a neutralizing agent of fatty acids to prepare soy soap and simultaneously release sulfur in sodium sulfide into an ultra fine sulfur powder and disperse the liberated sulfur powder naturally and uniformly without mechanical manipulation. I did it.
본 발명에서는 다음의 반응식 1과 같이 지방산을 황화나트륨으로 중화하여 비누를 제조한다.In the present invention, soap is prepared by neutralizing fatty acid with sodium sulfide as in Scheme 1 below.
위 반응식에서 황화나트륨은 다음의 반응식 2에서와 같이 2단계 반응에 의하여 수산화나트륨으로 전환되어 지방산과 반응하고 황화수소를 생성시킨다.In the above scheme, sodium sulfide is converted into sodium hydroxide by a two-step reaction as in Scheme 2 below to react with fatty acids and produce hydrogen sulfide.
위 반응식 2에서 생성된 황화수소 수용액은 불안정하여 다음의 반응식 3에서와 같이 공기중의 산소를 흡수하여 원소 유황을 유리한다.The hydrogen sulfide aqueous solution generated in Scheme 2 above is unstable and absorbs oxygen in the air to liberate elemental sulfur as shown in Scheme 3 below.
위 반응식에서 반응을 촉진하기 위하여 공기를 취입(吹入)하거나 코발트 몰리브데이트와 같은 산화촉매를 사용한다.In the above scheme, in order to promote the reaction, air is blown or an oxidation catalyst such as cobalt molybdate is used.
그러나 반응물중에 글리세린의 양이 지나치게 많으면 위 반응의 진행은 방해받게 된다.However, if the amount of glycerin in the reaction is too large, the progress of the above reaction is hampered.
또 유황비누의 유황 함량을 줄이기 위하여는 황화나트륨의 일부를 수산화나트륨으로 대체하면 된다.In order to reduce the sulfur content of sulfur soap, a part of sodium sulfide may be replaced with sodium hydroxide.
본 발명을 더욱 상세하게 설명하면 다음과 같다.The present invention is described in more detail as follows.
먼저 지방산과 글리세린 및 폴리에틸렌글리콜 혼합액(50:50wt%)을 반응기에 넣고 90°∼100℃의 온도로 30분간 가열한다.First, a mixture of fatty acid, glycerin, and polyethylene glycol (50:50 wt%) is added to a reactor and heated at a temperature of 90 ° to 100 ° C. for 30 minutes.
여기서 글리세린 및 폴리에틸렌글리콜 혼합액은 비누화시 조기응결을 방지하는 역할을 한다.Here, glycerin and polyethylene glycol mixed solution serves to prevent premature coagulation during saponification.
지방산 대 글리세린 및 폴리에틸렌글리콜 혼합액은 무게비율로 5:1∼10:1 정도로 사용한다.Fatty acid to glycerin and polyethylene glycol mixtures are used in weight ratios of about 5: 1 to 10: 1.
다음, 90°∼100℃의 온도에서 반응물을 교반하면서 30분간 70℃의 황화나트륨 10% 수용액을 서서히 주입한다.Next, a 10% aqueous solution of sodium sulfide at 70 ° C. is slowly injected for 30 minutes while stirring the reaction at a temperature of 90 ° to 100 ° C.
여기서 유황분말 유리를 촉진하기 위하여 공기를 취입하는 것이 바람직하다.Here, it is preferable to blow in air in order to promote the sulfur powder glass.
지방산과 황화나트륨은 지방산 1당량에 대하여 황화나트륨 0.6 당량 내외를 사용한다.Fatty acid and sodium sulfide are used at about 0.6 equivalents of sodium sulfide based on 1 equivalent of fatty acid.
다음, 90°∼100℃의 온도에서 황화수소의 냄새가 나지 않을때까지 더 교반한후 반응을 종결한 다음 통상적인 방법으로 염석(鹽析) 및 세척을 여러번하여 유황비누를 제조한다.Next, the mixture is further stirred until the smell of hydrogen sulfide is no longer smelled at a temperature of 90 ° to 100 ° C., and then the reaction is terminated, followed by salting and washing in a conventional manner to prepare sulfur soap.
실시예 1Example 1
우지증류지방산 300g과 글리세린 및 폴리에틸렌글리콜 50:50wt% 혼합액 30g을 반응기(ø230㎜, 높이 165㎜)에 넣고 95℃의 온도에서 30분간 가열한 다음, 95℃의 온도에서 반응물을 200rpm 으로 교반하여서 30분간 70℃의 황화나트륨 10% 수용액 500㎖ 를 서서히 주입한후 역시 95℃의 온도에서 200rpm 으로 황화수소의 냄새가 나지 않을때까지 더 교반한 다음 통상적인 방법으로 염석 및 세척을 여러번 하여 수분함량 16.6%의 유황비누 380g을 제조하였다.300 g of distilled fatty acid and 30 g of glycerin and polyethylene glycol 50:50 wt% mixed solution were added to a reactor (ø230 mm, height 165 mm), heated at a temperature of 95 ° C. for 30 minutes, and the reaction was stirred at 200 rpm at a temperature of 95 ° C., 30 After slowly injecting 500ml of sodium sulfide 10% aqueous solution at 70 ℃ for 200 minutes, further stirred at 95rpm at 200rpm until there is no smell of hydrogen sulfide, followed by salting and washing as usual, and water content 16.6% 380 g of sulfur soap was prepared.
실시예 2Example 2
우지증류지방산 300g과 글리세린 및 폴리에틸렌글리콜 50:50wt% 혼합액 30g을 반응기(ø230㎜, 높이 165㎜)에 넣고 95℃의 온도에서 30분간 가열한 다음, 95℃의 온도로 예열된 공기를 15.8ℓ/분의 양으로 취입하면서 동시에 95℃의 온도에서 200rpm 으로 반응물을 교반하면서 30분간 70℃의 황화나트륨 10% 수용액 500㎖를 서서히 주입한후 역시 95℃의 온도로 예열된 공기를 15.8ℓ/분의 양으로 취입하면서 동시에 95℃의 온도에서 황화수소의 냄새가 나지 않을때까지 200rpm 으로 반응물을 더 교반한 다음 통상적인 방법으로 염석 및 세척을 여러번 하여 수분함량 16.8% 의 유황비누 381g을 제조하였다.300 g of distilled fatty acid and 30 g of glycerin and polyethylene glycol 50:50 wt% mixed solution were added to a reactor (ø230 mm, height 165 mm), heated at a temperature of 95 ° C. for 30 minutes, and the air preheated to a temperature of 95 ° C. was 15.8 L / While slowly blowing 500 ml of sodium sulfide 10% aqueous solution at 70 ° C. for 30 minutes while stirring the reaction at 200 rpm at a temperature of 95 ° C. at a temperature of 95 ° C., the air preheated to a temperature of 95 ° C. was 15.8 L / min. At the same time, the reaction mixture was further stirred at 200 rpm until no smell of hydrogen sulfide was obtained at a temperature of 95 ° C., followed by salting and washing in a conventional manner, to prepare 381 g of sulfur soap having a water content of 16.8%.
본 발명의 실시예들에서 제조한 유황비누의 분석결과는 다음 표 1과 같았다.The analysis results of sulfur soaps prepared in Examples of the present invention were as shown in Table 1 below.
※ 기초과학지원연구소 부산분소의 분석결과임※ Result of analysis of Busan Branch of Basic Research Institute
본 발명에서는 유황을 화학적 방법으로 소지비누에 유리시킴으로써 초미립의 유황분말을 얻을 수 있었고 초미립의 유황분말을 소지비누에 자연발생적으로 균일하게 분산할 수 있도록 하여 초미립의 유황분말로 인하여 유황비누의 약효를 증대시킬 수 있었다.In the present invention, sulfur can be obtained in the soap by chemical method to obtain ultrafine sulfur powder, and the ultrafine sulfur powder can be naturally and uniformly dispersed in the soap by the ultrafine sulfur powder. Drug efficacy could be increased.
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KR101973935B1 (en) * | 2018-07-11 | 2019-04-30 | 황기철 | Complex sulfur with improved skin care effect and soap containing complex sulfur |
KR101973936B1 (en) * | 2018-07-11 | 2019-04-30 | 황기철 | Method for producing soap containing complex sulfur and mineral |
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